Supplementary Material (ESI) for Chemical Communications This journal is (C) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 182 # 1. SUBMISSION DETAILS _publ_contact_author 'Dr M Angeles Monge' _publ_contact_author_address ; A. Monge Instituto de Ciencia de Materiales CSIC Campus de Cantoblanco 28049 MADRID Spain ; _publ_contact_author_phone '34 1 334-9025' _publ_contact_author_fax '34 1 372-0623' _publ_contact_author_email amonge@icmm.csic.es _publ_requested_journal 'Chem. Commun.' _publ_requested_coeditor_name ? _publ_contact_letter ; ? ; #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Coopertive directing effect of OH anions and polymerized DABCO cations in the formation of the Ge16O32(OH)-(C6H12N2H)+(C6H12N2)(H2O)1.12 zeotype ; loop_ _publ_author_name _publ_author_address 'Manuela E. Medina' ; Instituto de Ciencia de Materiales CSIC Campus de Cantoblanco 28049 MADRID Spain ; 'Marta Iglesias' ; Instituto de Ciencia de Materiales CSIC Campus de Cantoblanco 28049 MADRID Spain ; 'Enrique Gutierrez-Puebla' ; Instituto de Ciencia de Materiales CSIC Campus de Cantoblanco 28049 MADRID Spain ; 'Maria Angeles Monge' ; Instituto de Ciencia de Materiales CSIC Campus de Cantoblanco 28049 MADRID Spain ; #============================================================================== # 4. TEXT _publ_section_abstract ; ; _publ_section_comment ; ; _publ_section_experimental ; ; _publ_section_references ; ; _publ_section_figure_captions ; ; _publ_section_acknowledgements ; ; #========================================================================= data_mm5 _database_code_CSD 168740 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'Ge16 O32 (OH) (C12 H25 N4) (H2 O)1.125' _chemical_formula_weight 1936.76 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Ge' 'Ge' 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I4(1)/amd loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+1/4, x+3/4, z+1/4' 'y+1/4, -x+1/4, z+3/4' '-x+1/2, y, -z+1/2' 'x, -y, -z' 'y+1/4, x+3/4, -z+1/4' '-y+1/4, -x+1/4, -z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+3/4, x+5/4, z+3/4' 'y+3/4, -x+3/4, z+5/4' '-x+1, y+1/2, -z+1' 'x+1/2, -y+1/2, -z+1/2' 'y+3/4, x+5/4, -z+3/4' '-y+3/4, -x+3/4, -z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-1/4, -x-3/4, -z-1/4' '-y-1/4, x-1/4, -z-3/4' 'x-1/2, -y, z-1/2' '-x, y, z' '-y-1/4, -x-3/4, z-1/4' 'y-1/4, x-1/4, z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y+1/4, -x-1/4, -z+1/4' '-y+1/4, x+1/4, -z-1/4' 'x, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' '-y+1/4, -x-1/4, z+1/4' 'y+1/4, x+1/4, z-1/4' _cell_length_a 25.973(2) _cell_length_b 25.973(2) _cell_length_c 27.088(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 18274(2) _cell_formula_units_Z 16 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.938 _exptl_crystal_density_method ? _exptl_crystal_F_000 10058 _exptl_absorpt_coefficient_mu 7.189 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 47517 _diffrn_reflns_av_R_equivalents 0.0984 _diffrn_reflns_av_sigmaI/netI 0.0915 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 3.51 _diffrn_reflns_theta_max 28.31 _reflns_number_total 5909 _reflns_number_observed 3544 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SMART V5.04 Bruker 1998' _computing_cell_refinement 'SAINT V5.04 Bruker 1998' _computing_data_reduction 'SAINT V5.04 Bruker 1998' _computing_structure_solution 'SHELXTL (Bruker, 1998)' _computing_structure_refinement 'SHELXTL (Bruker, 1998)' _computing_molecular_graphics 'SHELXTL (Bruker, 1998)' _computing_publication_material 'SHELXTL (Bruker, 1998)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0992P)^2^+107.2897P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom and difmap for O19' _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5909 _refine_ls_number_parameters 232 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1418 _refine_ls_R_factor_obs 0.0548 _refine_ls_wR_factor_all 0.1906 _refine_ls_wR_factor_obs 0.1588 _refine_ls_goodness_of_fit_all 1.018 _refine_ls_goodness_of_fit_obs 1.098 _refine_ls_restrained_S_all 1.018 _refine_ls_restrained_S_obs 1.098 _refine_ls_shift/esd_max 0.460 _refine_ls_shift/esd_mean 0.083 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ge1 Ge 0.16224(4) 0.58776(4) 1.1250 0.0108(3) Uani 1 d S 1 Ge2 Ge 0.19753(5) 0.68883(5) 0.81415(4) 0.0132(3) Uani 1 d . 1 Ge3 Ge 0.06087(5) 0.56704(5) 0.95130(4) 0.0111(3) Uani 1 d . 1 Ge4 Ge 0.18252(5) 0.68922(5) 0.69981(4) 0.0133(3) Uani 1 d . 1 Ge5 Ge 0.06133(4) 0.55305(5) 1.06602(4) 0.0107(3) Uani 1 d . 1 Ge6 Ge 0.14763(5) 0.60237(5) 0.6250 0.0141(4) Uani 1 d S 1 Ge7 Ge 0.23812(5) 0.56394(4) 0.55596(4) 0.0134(3) Uani 1 d . 1 Ge8 Ge 0.15672(5) 0.59478(5) 0.88694(4) 0.0141(3) Uani 1 d . 1 Ge9 Ge 0.25933(5) 0.55513(5) 1.05724(4) 0.0154(3) Uani 1 d . 1 O1 O 0.0000 0.5548(6) 1.0919(4) 0.030(3) Uani 1 d S 1 O2 O 0.0000 0.5775(6) 0.9278(5) 0.033(4) Uani 1 d S 1 O3 O 0.1949(3) 0.5703(3) 1.0718(3) 0.023(2) Uani 1 d . 1 O4 O 0.1642(4) 0.6530(4) 0.8583(4) 0.030(2) Uani 1 d . 1 O5 O 0.0964(3) 0.5831(3) 1.1120(3) 0.018(2) Uani 1 d . 1 O6 O 0.1387(3) 0.6536(3) 0.6658(3) 0.026(2) Uani 1 d . 1 O7 O 0.0973(3) 0.6079(3) 0.9155(3) 0.018(2) Uani 1 d . 1 O8 O 0.0666(4) 0.5885(4) 1.0128(3) 0.025(2) Uani 1 d . 1 O9 O 0.1747(5) 0.7500 0.6749(5) 0.033(4) Uani 1 d S 1 O10 O 0.1615(4) 0.6835(4) 0.7599(3) 0.029(2) Uani 1 d . 1 O11 O 0.2041(3) 0.6097(3) 0.5914(3) 0.019(2) Uani 1 d . 1 O12 O 0.0884(3) 0.5072(3) 0.9409(3) 0.026(2) Uani 1 d . 1 O13 O 0.2156(3) 0.5036(3) 0.5772(3) 0.019(2) Uani 1 d . 1 O14 O 0.1526(3) 0.5421(4) 0.8482(3) 0.024(2) Uani 1 d . 1 O15 O 0.2178(3) 0.5830(3) 0.4969(3) 0.018(2) Uani 1 d . 1 O16 O 0.3019(3) 0.5843(3) 0.5648(3) 0.019(2) Uani 1 d . 1 O17 O 0.2580(4) 0.6614(3) 0.8096(4) 0.032(2) Uani 1 d . 1 O18 O 0.1959(6) 0.7500 0.8395(5) 0.029(3) Uani 1 d S 1 O19 O 0.2225(5) 0.5000 1.0000 0.049(4) Uani 1 d S 1 H19 N 0.1908 0.5000 1.0000 0.070 Uiso 0.00 d SP 1 N1 N 0.2481 0.7500 0.4951 0.078 Uiso 1 d S . N2 N 0.1520 0.7500 0.4908 0.073 Uiso 1 d S . N3 N 0.6480 0.7500 0.4994 0.077 Uiso 1 d S . N4 N 0.5570 0.7500 0.4989 0.050 Uiso 1 d S . C2 C 0.1755 0.8002 0.4766 0.107 Uiso 1 d . . H21 H 0.1589 0.7916 0.4492 0.050 Uiso 1 d R . H22 H 0.1629 0.8395 0.4866 0.050 Uiso 1 d R . C3 C 0.1811 0.7500 0.5472 0.106 Uiso 1 d S . H3A H 0.1681 0.7799 0.5647 0.127 Uiso 0.50 calc PR . H3B H 0.1681 0.7201 0.5647 0.127 Uiso 0.50 calc PR . C4 C 0.2358 0.7500 0.5538 0.106 Uiso 1 d S . H4A H 0.2483 0.7193 0.5704 0.127 Uiso 0.50 calc PR . H4B H 0.2483 0.7807 0.5704 0.127 Uiso 0.50 calc PR . C5 C 0.6428 0.7500 0.5510 0.106 Uiso 1 d S . H5A H 0.6577 0.7805 0.5659 0.127 Uiso 0.50 calc PR . H5B H 0.6577 0.7195 0.5659 0.127 Uiso 0.50 calc PR . C7 C 0.6294 0.7991 0.4764 0.108 Uiso 1 d . . H7A H 0.6412 0.8014 0.4425 0.130 Uiso 1 calc R . H7B H 0.6427 0.8285 0.4944 0.130 Uiso 1 calc R . C8 C 0.5669 0.7989 0.4782 0.105 Uiso 1 d . . H8A H 0.5538 0.8264 0.4989 0.125 Uiso 1 calc R . H8B H 0.5522 0.8021 0.4454 0.125 Uiso 1 calc R . C6 C 0.5764 0.7500 0.5543 0.147 Uiso 1 d S . H6A H 0.5642 0.7196 0.5715 0.176 Uiso 0.50 calc PR . H6B H 0.5642 0.7804 0.5715 0.176 Uiso 0.50 calc PR . C1 C 0.2294 0.8003 0.4734 0.183 Uiso 1 d . . H1A H 0.2435 0.8291 0.4917 0.220 Uiso 1 calc R . H1B H 0.2402 0.8032 0.4392 0.220 Uiso 1 calc R . O1W O 0.2500 0.7500 0.7500 0.027(4) Uiso 1 d S . O2W O 0.0000 0.5000 0.0000 0.031(4) Uiso 1 d S . O3W O 0.0000 0.7500 0.6250 0.062(9) Uiso 1 d S . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ge1 0.0110(5) 0.0110(5) 0.0102(7) -0.0016(5) -0.0016(5) -0.0005(6) Ge2 0.0126(6) 0.0147(6) 0.0123(6) 0.0038(5) 0.0012(5) 0.0001(5) Ge3 0.0102(6) 0.0126(6) 0.0105(6) 0.0008(5) 0.0009(5) -0.0004(4) Ge4 0.0129(6) 0.0137(6) 0.0133(6) -0.0044(5) -0.0009(5) -0.0007(5) Ge5 0.0090(6) 0.0131(6) 0.0101(6) -0.0003(5) -0.0002(4) -0.0006(4) Ge6 0.0148(5) 0.0148(5) 0.0128(7) -0.0030(5) -0.0030(5) 0.0010(6) Ge7 0.0151(7) 0.0147(6) 0.0105(5) 0.0014(4) -0.0017(4) -0.0032(5) Ge8 0.0103(6) 0.0198(7) 0.0121(5) 0.0052(5) 0.0000(5) -0.0010(5) Ge9 0.0199(7) 0.0151(6) 0.0113(6) 0.0028(4) 0.0051(5) 0.0043(5) O1 0.027(8) 0.049(9) 0.015(6) -0.009(6) 0.000 0.000 O2 0.004(6) 0.061(10) 0.035(8) 0.028(7) 0.000 0.000 O3 0.015(4) 0.033(5) 0.021(4) -0.006(4) 0.003(4) 0.000(4) O4 0.025(5) 0.025(5) 0.039(6) 0.012(4) 0.008(4) -0.001(4) O5 0.010(4) 0.032(5) 0.011(4) -0.009(4) -0.002(3) -0.003(3) O6 0.013(5) 0.029(5) 0.034(5) -0.025(4) -0.002(4) -0.004(4) O7 0.016(4) 0.021(5) 0.017(4) 0.003(4) 0.001(3) -0.001(3) O8 0.032(5) 0.031(6) 0.013(4) -0.001(4) -0.002(4) -0.011(4) O9 0.034(8) 0.023(8) 0.041(8) 0.000 -0.030(7) 0.000 O10 0.033(6) 0.030(5) 0.024(5) -0.005(4) 0.000(4) -0.007(4) O11 0.028(5) 0.014(4) 0.017(4) -0.006(3) 0.008(4) -0.008(4) O12 0.024(5) 0.014(5) 0.039(5) -0.009(4) 0.013(4) -0.002(4) O13 0.026(4) 0.015(4) 0.017(4) -0.002(3) 0.003(3) -0.006(4) O14 0.022(5) 0.036(6) 0.015(4) -0.011(4) -0.001(4) -0.002(4) O15 0.029(5) 0.018(4) 0.007(3) -0.002(3) -0.008(4) 0.004(3) O16 0.020(5) 0.026(5) 0.010(4) -0.006(3) -0.002(3) -0.005(4) O17 0.020(5) 0.023(5) 0.052(6) 0.013(4) 0.000(5) -0.001(4) O18 0.044(9) 0.013(6) 0.029(7) 0.000 0.011(7) 0.000 O19 0.008(6) 0.065(11) 0.073(11) 0.013(9) 0.000 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ge1 O3 1.732(8) . ? Ge1 O3 1.732(8) 16_556 ? Ge1 O5 1.750(8) . ? Ge1 O5 1.750(8) 16_556 ? Ge2 O18 1.731(5) . ? Ge2 O17 1.729(9) . ? Ge2 O4 1.744(9) . ? Ge2 O10 1.748(9) . ? Ge3 O2 1.725(5) . ? Ge3 O7 1.723(8) . ? Ge3 O12 1.733(9) . ? Ge3 O8 1.764(8) . ? Ge4 O10 1.724(9) . ? Ge4 O17 1.725(9) 5_556 ? Ge4 O9 1.729(5) . ? Ge4 O6 1.732(8) . ? Ge5 O8 1.715(8) . ? Ge5 O12 1.726(9) 6_567 ? Ge5 O5 1.730(7) . ? Ge5 O1 1.741(5) . ? Ge6 O11 1.736(8) 16 ? Ge6 O11 1.736(8) . ? Ge6 O6 1.745(8) . ? Ge6 O6 1.745(8) 16 ? Ge7 O15 1.755(8) . ? Ge7 O11 1.764(8) . ? Ge7 O16 1.756(8) . ? Ge7 O13 1.769(8) . ? Ge8 O16 1.714(8) 5_556 ? Ge8 O4 1.710(9) . ? Ge8 O14 1.727(9) . ? Ge8 O7 1.759(8) . ? Ge9 O15 1.741(8) 5_556 ? Ge9 O13 1.745(9) 2_565 ? Ge9 O3 1.764(8) . ? Ge9 O14 1.778(9) 12_454 ? Ge9 O19 2.317(6) . ? O1 Ge5 1.741(5) 22 ? O2 Ge3 1.725(5) 22 ? O9 Ge4 1.729(6) 29_565 ? O12 Ge5 1.726(9) 6_567 ? O13 Ge9 1.745(9) 2_564 ? O14 Ge9 1.778(8) 11_544 ? O15 Ge9 1.741(8) 5_556 ? O16 Ge8 1.714(8) 5_556 ? O17 Ge4 1.725(9) 5_556 ? O18 Ge2 1.731(5) 29_565 ? O19 H19 0.824(13) . ? O19 Ge9 2.317(5) 6_567 ? N1 C1 1.5131(1) 29_565 ? N1 C1 1.5131(1) . ? N1 C4 1.6196(1) . ? N2 C2 1.4912(1) . ? N2 C2 1.4912(1) 29_565 ? N2 C3 1.7048(1) . ? N3 C5 1.4028(1) . ? N3 C7 1.4992(1) 29_565 ? N3 C7 1.4992(1) . ? N4 C8 1.4135(1) 29_565 ? N4 C8 1.4135(1) . ? N4 C6 1.5829(1) . ? C2 C1 1.4021(1) . ? C3 C4 1.4320(1) . ? C5 C6 1.7283(1) . ? C7 C8 1.6225(1) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Ge1 O3 115.8(6) . 16_556 ? O3 Ge1 O5 107.0(4) . . ? O3 Ge1 O5 112.9(4) 16_556 . ? O3 Ge1 O5 112.9(4) . 16_556 ? O3 Ge1 O5 107.0(4) 16_556 16_556 ? O5 Ge1 O5 100.2(6) . 16_556 ? O18 Ge2 O17 115.4(6) . . ? O18 Ge2 O4 101.9(5) . . ? O17 Ge2 O4 106.2(4) . . ? O18 Ge2 O10 113.1(6) . . ? O17 Ge2 O10 113.2(5) . . ? O4 Ge2 O10 105.5(5) . . ? O2 Ge3 O7 101.5(5) . . ? O2 Ge3 O12 117.3(6) . . ? O7 Ge3 O12 103.5(4) . . ? O2 Ge3 O8 112.1(6) . . ? O7 Ge3 O8 107.0(4) . . ? O12 Ge3 O8 113.7(5) . . ? O10 Ge4 O17 112.8(5) . 5_556 ? O10 Ge4 O9 114.2(6) . . ? O17 Ge4 O9 115.5(6) 5_556 . ? O10 Ge4 O6 104.4(4) . . ? O17 Ge4 O6 106.6(4) 5_556 . ? O9 Ge4 O6 101.7(5) . . ? O8 Ge5 O12 111.3(5) . 6_567 ? O8 Ge5 O5 108.7(4) . . ? O12 Ge5 O5 105.8(4) 6_567 . ? O8 Ge5 O1 113.4(5) . . ? O12 Ge5 O1 116.1(6) 6_567 . ? O5 Ge5 O1 100.4(5) . . ? O11 Ge6 O11 117.3(6) 16 . ? O11 Ge6 O6 107.3(4) 16 . ? O11 Ge6 O6 111.1(4) . . ? O11 Ge6 O6 111.1(4) 16 16 ? O11 Ge6 O6 107.3(4) . 16 ? O6 Ge6 O6 101.4(6) . 16 ? O15 Ge7 O11 98.9(4) . . ? O15 Ge7 O16 108.9(4) . . ? O11 Ge7 O16 101.3(4) . . ? O15 Ge7 O13 116.5(4) . . ? O11 Ge7 O13 104.7(4) . . ? O16 Ge7 O13 122.3(4) . . ? O16 Ge8 O4 114.6(4) 5_556 . ? O16 Ge8 O14 112.1(4) 5_556 . ? O4 Ge8 O14 115.5(5) . . ? O16 Ge8 O7 104.2(4) 5_556 . ? O4 Ge8 O7 97.3(4) . . ? O14 Ge8 O7 111.5(4) . . ? O15 Ge9 O13 119.8(4) 5_556 2_565 ? O15 Ge9 O3 114.8(4) 5_556 . ? O13 Ge9 O3 118.7(4) 2_565 . ? O15 Ge9 O14 96.1(4) 5_556 12_454 ? O13 Ge9 O14 99.7(4) 2_565 12_454 ? O3 Ge9 O14 100.2(4) . 12_454 ? O15 Ge9 O19 80.4(3) 5_556 . ? O13 Ge9 O19 79.7(3) 2_565 . ? O3 Ge9 O19 84.0(4) . . ? O14 Ge9 O19 175.4(4) 12_454 . ? Ge5 O1 Ge5 132.4(7) . 22 ? Ge3 O2 Ge3 132.8(8) . 22 ? Ge1 O3 Ge9 135.2(5) . . ? Ge8 O4 Ge2 147.1(6) . . ? Ge5 O5 Ge1 133.7(5) . . ? Ge4 O6 Ge6 131.1(5) . . ? Ge3 O7 Ge8 127.6(5) . . ? Ge5 O8 Ge3 128.1(5) . . ? Ge4 O9 Ge4 131.9(8) . 29_565 ? Ge4 O10 Ge2 128.1(6) . . ? Ge6 O11 Ge7 129.4(5) . . ? Ge3 O12 Ge5 131.5(5) . 6_567 ? Ge9 O13 Ge7 123.4(5) 2_564 . ? Ge8 O14 Ge9 136.0(5) . 11_544 ? Ge9 O15 Ge7 123.2(5) 5_556 . ? Ge8 O16 Ge7 138.0(5) 5_556 . ? Ge4 O17 Ge2 130.6(5) 5_556 . ? Ge2 O18 Ge2 133.1(8) . 29_565 ? H19 O19 Ge9 114.4(3) . . ? H19 O19 Ge9 114.4(3) . 6_567 ? Ge9 O19 Ge9 131.3(6) . 6_567 ? C1 N1 C1 119.410(3) 29_565 . ? C1 N1 C4 108.596(3) 29_565 . ? C1 N1 C4 108.596(2) . . ? C2 N2 C2 122.100(1) . 29_565 ? C2 N2 C3 92.866(2) . . ? C2 N2 C3 92.866(2) 29_565 . ? C5 N3 C7 112.551(3) . 29_565 ? C5 N3 C7 112.551(3) . . ? C7 N3 C7 116.488(5) 29_565 . ? C8 N4 C8 128.131(5) 29_565 . ? C8 N4 C6 108.572(3) 29_565 . ? C8 N4 C6 108.571(3) . . ? C1 C2 N2 115.2 . . ? C4 C3 N2 123.406(2) . . ? C3 C4 N1 94.241(2) . . ? N3 C5 C6 98.5 . . ? N3 C7 C8 107.9 . . ? N4 C8 C7 101.3 . . ? N4 C6 C5 105.558(2) . . ? C2 C1 N1 107.1 . . ? _refine_diff_density_max 2.465 _refine_diff_density_min -3.872 _refine_diff_density_rms 0.245